Novel techniques of capillary liquid chromatography are under development. The chromatorgraphic micro-columns are prepared by drawing small adsorbent particles into glass capillaries under the heat of glass melting. Adsorbents are either siliceous and alumina materials, that can be further reacted with various silane compounds to form chemically bonded phases of different selectives. Flow-rates through such columns are of the order of a few microliters per minute, making them ideal for columns are of the order of a few microliters per minute, making them ideal for LC/MS and LC/IR combinations. LC capillary columns have efficiencies in the range of 10 to the fifth power to 10 to the sixth power theoretical plates. Potential and limitations of high pressures (around 1000 atmospheres) in achieving extremely high efficiencies will be explored. Several unique detection devices will be developed (to be compatible with capillary LC), including small-volume (below 0.1 microliter cell) electrochmical and spectrofluorometric detectors, the flame photometric and themionic detectors.